CN102350291A - Reactor for gas phase modified nano-powder body - Google Patents

Reactor for gas phase modified nano-powder body Download PDF

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Publication number
CN102350291A
CN102350291A CN2011102576303A CN201110257630A CN102350291A CN 102350291 A CN102350291 A CN 102350291A CN 2011102576303 A CN2011102576303 A CN 2011102576303A CN 201110257630 A CN201110257630 A CN 201110257630A CN 102350291 A CN102350291 A CN 102350291A
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China
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reactor
agitator
modified nano
vapor phase
phase method
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CN2011102576303A
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Chinese (zh)
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任真
王玲玲
郭建平
赵永红
李玉霞
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China Daily Chemical Industry Research Institute
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China Daily Chemical Industry Research Institute
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Abstract

The invention discloses a reactor for a gas phase modified nano-powder body. The reactor comprises an upper-layer baffle plate, a lower-layer supporting plate and a stirring device, wherein the upper-layer baffle plate is of a high temperature micropore ceramic plate structure; in the upper-layer baffle plate, the aperture is 10 to 200 microns, the aperture ratio is 30-50%, the air permeability is less than or equal to 2.5 m<3>/m<2> and the heat resistance temperature is 800 DEG C; the lower-layer supporting plate is of a high temperature micropore ceramic plate structure; in the lower-layer supporting plate, the aperture is 10 to 500 microns, the aperture ratio is 30-50%, the air permeability is less than or equal to 2.5 m<3>/m<2> and the heat resistance temperature is 800 DEG C; the stirring device is positioned between the upper-layer baffle plate and the lower-layer supporting plate; and the stirring device consists of a first stirrer and a second stirrer which are connected with each other in a shafted manner. The reactor modifies nano-powder body particles by controlling the use amount of modifier, modification temperature and modification time, therefore, the problems of non-uniformity and uncontrollability of modification of nano materials are solved.

Description

A kind of reactor that is used for the vapor phase method modified nano powder
Technical field
The present invention is relevant with a kind of device of nano-powder material modification, says further, is the reactor that comprises a kind of vapor phase method modified nano powder of agitated reactor, electrical heating cover, feed inlet and outlet, air inlet/outlet and agitating device.
Background technology
In the preparation classification and application process of nano material; The dispersion treatment of carrying out for the dispersiveness that improves powder; Be activity that improves powder and the activation processing that compatibility is carried out; And the ion Combined Processing of carrying out for the function of use that improves powder, be commonly referred to the surface modification treatment of nano material.Product to after pulverizing carries out surface modification treatment; Belong to dry method modification; Be about to nano-powder and modifier and add in the modified device, adopt mechanical system to stir at a certain temperature, make its surface that surface modifier adsorbs or adhere to the powder that is modified in mixed process; And under the effect that adds mechanical force, make between them and combine closely, and then reach the modification purpose.Adopt the employed modified device of this technology to mainly contain: high-speed stirring mixer, high speed kneader, mixer, fixed bed, fluid bed, medium stirring ball-milling, vibromill and agitated reactor etc.Reactor among the present invention and fixed bed reactors and fluidized-bed reactor have similar part.
Fixed bed reactors have three kinds of citation forms: 1. axial heat-insulating fixed bed reactors.The fluid bed of flowing through from top to bottom vertically, bed is with extraneous no heat exchange.2. radial adiabatic formula fixed bed reactors.Fluid radially flows through bed, can adopt centrifugal flow or entad flow the together extraneous no heat exchange of bed.Radial reactor is compared with axial flow reactor, and the distance that fluid flows is shorter, and cross section of fluid channel is long-pending bigger, and the pressure of fluid falls less.But the structure of radial reactor is complicated than axial flow reactor.More than two kinds of forms all belong to adiabatic reactor, be applicable to that reaction heat effect is little, or reaction system can bear the occasion of the variations in temperature that is caused by reaction heat effect under the adiabatic condition.3. calandria type fixed bed reactor.Constitute by many reaction tube parallel connections.Put solid formation in the pipe or between pipe, heat or cool off between the thermophore flowing pipe or in the pipe, caliber between 25~50mm, is managed number and can be reached up to ten thousand usually.Calandria type fixed bed reactor is applicable to the reaction that reaction heat effect is bigger.In addition, the reactor that is formed by above-mentioned citation form tandem compound is arranged still, be called multistage fixed bed reactor, establish heat exchanger or additional material between the reactor regulating temperature, so that operate under the optimal temperature conditions approaching.
The advantage of fixed bed reactors is: 1. back-mixing is little, and fluid can effectively contact with solid phase, can be than high selectivity when reacting with the series connection side reaction.2. simple in structure.The shortcoming of fixed bed reactors is: it is poor to conduct heat, when the exothermic heat of reaction amount is very big, even temperature runaway (reaction temperature is out of hand, sharply rises, and surpasses allowed band) also possibly appear in shell and tube reactor.
Fluidized-bed reactor is the Winkler stove that is applied as the coal gasification that occurs the twenties in 20th century in early days in the industry in modern times; But the developing of modern fluidized reaction technology, with the forties petroleum catalytic cracking be representative.At present, fluidized-bed reactor is used widely in departments such as chemical industry, oil, metallurgy, nuclear industry.The structure of fluidized-bed reactor has two kinds of forms: 1. solid material continuous feed and drawing mechanism are arranged, be used for the fluid phase process of solid phase process or rapid catalyst deactivation.2. do not have solid material continuous feed and drawing mechanism, be used for the solid particle proterties in the long duration, the course of reaction of significant change does not take place.
Compare with fixed bed reactors, the advantage of fluidized-bed reactor is: 1. can realize the continuous input and output of solid material; 2. the motion of fluid and particle makes bed have the good heat transfer performance, and the bed internal temperature is even, and is easy to control, is specially adapted to strong exothermal reaction.But then, because back-mixing is serious, can bring certain influence to the efficient of reactor and the selectivity of reaction.The existence of adding gas-solid fluidized bed middle bubble makes and gas-solid contact variation causes gas reaction to get not exclusively.Therefore, should not be used for the very high reaction of requirement conversion per pass usually.In addition, the wearing and tearing of solid particle and the dust in the air-flow are carried secretly, also make the application of fluid bed receive certain limitation.
In recent years, all existing commercial Application of the turbulent fluidized bed of fine grained and high gas speed and high-velocity fluidized bed.Under the condition of particle entrainment speed, the circulation through solid to be keeping bed in high cycle speed, owing to strengthened the alternate contact of gas-solid two, is particularly conducive to the situation that the interphase mass transfer resistance occupies critical role.Because a large amount of solid particles is carried secretly by gas, need separate and recycle and return bed but then, therefore, also just very high to the requirement of gas solid separation.
The present invention is used for the reactor of modified nano powder particle, with respect to fixed bed reactors, in reactor, has increased the agitating device of being made up of jointly dasher and helical ribbon agitator, increases heat transfer efficiency, makes powder-modified more even; With respect to fluidized-bed reactor; This reactor has solved the difficult problem of fluid bed gas solid separation; The gripper shoe of reactor lower end and upper strata baffle plate all adopt capillary ceramic plate; The powder that can stop the overwhelming majority is stayed in the reactor, only has the agent that is modified of a small amount of powder to take out of, is collected by external cyclone separator.Intermittent reaction can be controlled the powder-modified homogeneity of temperature, gas-solid ratio, assurance in the reactor, through the control modification time, can control the coating thickness and the modified effect of modifier.
Summary of the invention
The present invention provides a kind of reactor that is used for the vapor phase method modified nano powder, and is existing nano powder modified inhomogeneous in order to solve, the uncontrollability problem of modified nano powder.
A kind of reactor that is used for the vapor phase method modified nano powder comprises upper strata baffle plate, lower layer support plate and agitating device;
Said upper strata baffle plate is a high temperature micropore ceramics plate structure, its aperture: 10 ~ 200 μ m; Percent opening: 30 ~ 50 %; Ventilative Shuai ≦ 2.5 m 3/ m 2H; Heat resisting temperature: 800 ° of C;
Said lower layer support plate is a high temperature micropore ceramics plate structure, its aperture: 10 ~ 500 μ m; Percent opening: 30 ~ 50 %; Ventilative Shuai ≦ 2.5 m 3/ m 2H; Heat resisting temperature: 800 ° of C;
Said agitating device is to be positioned between upper strata baffle plate and lower layer support plate, by first agitator and coaxial the connecting and composing of the second agitator two-stage agitator.
In technique scheme, said nano-powder is zinc oxide, magnesia, calcium carbonate, titanium dioxide, silica; Said first agitator is a helical ribbon agitator, be positioned at second agitator above, the height of its helical ribbon agitator is 1/2~2/3 of a kettle height, draw ratio is 1.5~3; Said second agitator is a dasher; Be positioned on the axis on the lower layer support plate, its dasher is that the gap with reactor wall is 3~10 cm, and the blade of dasher is provided with aperture; The diameter of its aperture is 5-10cm, and percent opening is 30%-50%;
A kind of reactor that is used for the modified nano powder particle of the present invention is compared with existing fixed bed reactors, in reactor, has increased the agitating device of being made up of jointly dasher and helical ribbon agitator, has increased heat transfer efficiency, makes powder-modified more even; With respect to fluidized-bed reactor; This reactor has solved the difficult problem of fluid bed gas solid separation; The gripper shoe of reactor lower end and upper strata baffle plate all adopt capillary ceramic plate; The powder that can stop the overwhelming majority is stayed in the reactor, only has the agent that is modified of a small amount of powder to take out of, is collected by external cyclone separator.Intermittent reaction can be controlled the powder-modified homogeneity of temperature, gas-solid ratio, assurance in the reactor, through the control modification time, can control the coating thickness and the modified effect of modifier.And adopt the method for vapor phase method modification, once can access modified product, removed the step of dry out solvent in the liquid phase method modification, reduced environmental pollution.
Description of drawings
Fig. 1 is the structural representation that the present invention is used for the modified nano powder reactor.
Among the figure: 1: charging aperture; 2: sample tap; 3: discharging opening; 4: air inlet; 5: the gas outlet; 6: the upper strata baffle plate; 7: the electrical heating cover; 8: temperature-measuring port; 9: the first agitators; 10: the second agitators; 11: the lower layer support plate.
The specific embodiment
Following specific embodiments of the invention is made an explanation.
The specific embodiment 1
Of Fig. 1; A kind of reactor that is used for the vapor phase method modified nano powder of embodiment of the present invention is made up of stainless steel kettle, outer electrical heating cover 7, charging aperture 1, discharging opening 3, air inlet 4, gas outlet 5, sample tap 2, lower layer support plate 11, upper strata baffle plate 6 and agitating device.What reactor was concrete is constructed as follows:
Reactor of the present invention adopts the stainless steel kettle, and draw ratio is 1.5-3, is fixed on the kettle by method indigo plant at the bottom of still top and the still; Kettle inside is provided with the draw-in groove of capillary ceramic plate up and down; Being provided with in the middle of the still top can be through stirring shaft seal; Charging aperture 1 is positioned at the kettle upper end, is lower than the 5-10cm of upper strata baffle plate 6 positions; Discharging opening 3 is positioned at the kettle lower end, with the flush of lower layer support plate 11; Kettle 2/3 to 3/4 place is provided with temperature-measuring port 8, diameter and temperature measuring equipment coupling; There is sample tap 2 at kettle 1/2 place, and diameter is 5-10 cm.
Described outer electrical heating cover 7 is to be wrapped in stainless steel kettle outer surface, and the heating-up temperature during work is 0-500 ° of C;
Described charging aperture 1 is a circular hole, connects feeding warehouse, and diameter is 10-20cm; Described discharging opening 3 is a square hole, and the flush of lower limb and lower layer support plate 11, the length of side are 10-20cm.
Described air inlet 4 and gas outlet 5 can be opened the optional position at the bottom of still top and still, and size is identical, and diameter is 10-20cm;
Said upper strata baffle plate 6 is to adopt high temperature micropore ceramics plate structure, and middle porose and sealing device is convenient to shaft and is passed through; Its aperture: 10 ~ 200 μ m; Percent opening: 30 ~ 50 %; Ventilative Shuai ≦ 2.5 m 3/ m 2H; Heat resisting temperature: 800 ° of C;
Said lower layer support plate 11 is to adopt high temperature micropore ceramics plate structure, its aperture: 10 ~ 500 μ m; Percent opening: 30 ~ 50 %; Ventilative Shuai ≦ 2.5 m 3/ m 2H; Heat resisting temperature: 800 ° of C;
Described agitating device is made up of first agitator 9 and second agitator 10.First agitator 9 is a helical ribbon agitator, occupies 1/2 to 2/3 of kettle height, draw ratio 1.5-3; Second agitator 10 is a dasher, and blade outward flange and agitated reactor distance are 3-10 cm, punch on the blade, and diameter is 5-10cm, and percent opening is 30%-50%; First agitator 9 and second agitator 10 belong to coaxial stirring, and rotating speed is 0-5000r/min.Can be out-of-alignment also, can adopt the speed changer rotating shaft to drive second agitator 10 during disalignment.Or second agitator 10 is fixed on the middle position of upper strata baffle plate 6, rotating speed can be adjusted between 0-5000r/min.
At the above-mentioned reactor that is used for the vapor phase method modified nano powder of the present invention, be applicable to that modified nano powder is zinc oxide, magnesia, calcium carbonate, titanium dioxide, silica.
Following specific embodiments of the invention is made further detailed description.
Embodiment 1
Of Fig. 1; A kind of reactor that is used for the vapor phase method modified nano powder that embodiment of the present invention provided comprises stainless steel kettle, outer electrical heating cover 7, charging aperture 1, discharging opening 3, air inlet 4, gas outlet 5, sample tap 2, temperature-measuring port 8, first agitator 9, second agitator 10, lower layer support plate 11 and upper strata baffle plate 6.
Add nano-powder from charging aperture 1,, open nitrogen cylinder, feed nitrogen, drive the air in the reactor away from air inlet 4 like nanometer Zinc oxide powder; Open first agitator 9 and second agitator 10 of the agitating device on the reactor, and outer electric heater unit 7, it is 100-350 ℃ that the nano-powder uniform particles is preheating to temperature; Boiling point according to different modifier; It is between 50-300 ℃ that modifier is heated to temperature; The temperature of promptly controlling in the reactor is higher than 10 ℃~50 ℃ of modifier vapor (steam) temperatures, utilizes nitrogen to carry, and the modifier steam is fed the reactor from air inlet 4; Through lower floor's capillary ceramic plate 11,, brute force fully contacts under stirring with the nano-powder of preheating.Certain hour takes out a certain amount of powder from sample tap 2 and detects at interval.Temperature and time through the control modification is controlled modified effect.Unreacted modifier steam, nitrogen and a small amount of powder see through upper strata baffle plate 6, through gas outlet 5, leave reactor, get into cyclone separator, carry out gas solid separation.By the powder of cyclone separator interception, after the cooling, it is qualified then as finished product packing to detect, if defective, correcting property under then participating in.In whole modifying process, modifier and nitrogen recycle in system, economic environment-friendly high-efficiency.

Claims (7)

1. a reactor that is used for the vapor phase method modified nano powder comprises upper strata baffle plate, lower layer support plate and agitating device;
Said upper strata baffle plate (6) is a high temperature micropore ceramics plate structure, its aperture: 10 ~ 200 μ m; Percent opening: 30 ~ 50 %; Ventilative Shuai ≦ 2.5 m 3/ m 2H; Heat resisting temperature: 800 ° of C;
Said lower layer support plate (11) is a high temperature micropore ceramics plate structure, its aperture: 10 ~ 500 μ m; Percent opening: 30 ~ 50 %; Ventilative Shuai ≦ 2.5 m 3/ m 2H; Heat resisting temperature: 800 ° of C;
Said agitating device is to be positioned between upper strata baffle plate (6) and lower layer support plate (11), by first agitator (9) and coaxial the connecting and composing of second agitator (10) two-stage agitator.
2. like the described a kind of reactor that is used for the vapor phase method modified nano powder of claim 1, said nano-powder is a kind of in zinc oxide, magnesia, calcium carbonate, titanium dioxide and the silica.
3. like the described a kind of reactor that is used for the vapor phase method modified nano powder of claim 1, said first agitator (9) is a helical ribbon agitator, be positioned at second agitator (10) above.
4. a kind of reactor that is used for the vapor phase method modified nano powder as claimed in claim 3, said helical ribbon agitator is 1/2~2/3 of a kettle height, draw ratio is 1.5~3.
5. like the described a kind of reactor that is used for the vapor phase method modified nano powder of claim 3, said second agitator (10) is a dasher, is positioned on the axis on the lower layer support plate (11).
6. like the described a kind of reactor that is used for the vapor phase method modified nano powder of claim 5, said dasher is that the gap with reactor wall is 3~10 cm.
7. a kind of reactor that is used for the vapor phase method modified nano powder as claimed in claim 5, the blade of said dasher is provided with aperture, and said hole diameter is 5-10cm, and percent opening is 30%-50%.
CN2011102576303A 2011-09-02 2011-09-02 Reactor for gas phase modified nano-powder body Pending CN102350291A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103721664A (en) * 2013-12-13 2014-04-16 中国科学院宁波材料技术与工程研究所 Device and method for modifying carbon material by gas
CN104741062A (en) * 2014-07-09 2015-07-01 季永东 Heat resistant type electrical heating reaction vessel
CN108878766A (en) * 2018-05-22 2018-11-23 桑德集团有限公司 For being modified the device and method of lithium-rich anode material
CN109161226A (en) * 2018-11-02 2019-01-08 巢湖学院 A kind of inorganic nanometer powder surface organic decorating device

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1579611A (en) * 2003-07-31 2005-02-16 中国石油化工股份有限公司 Gas-solid reaction equipment
CN1958145A (en) * 2005-11-04 2007-05-09 中国科学院过程工程研究所 Fluidized-bed reactor for oxidizing carbon black through ozone
CN201062168Y (en) * 2007-06-26 2008-05-21 北京航天万源煤化工工程技术有限公司 Powder solid fluidizing device
US20090126721A1 (en) * 2007-11-16 2009-05-21 Thomas Joseph English Continuous Fluid Bed Reactor

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1579611A (en) * 2003-07-31 2005-02-16 中国石油化工股份有限公司 Gas-solid reaction equipment
CN1958145A (en) * 2005-11-04 2007-05-09 中国科学院过程工程研究所 Fluidized-bed reactor for oxidizing carbon black through ozone
CN201062168Y (en) * 2007-06-26 2008-05-21 北京航天万源煤化工工程技术有限公司 Powder solid fluidizing device
US20090126721A1 (en) * 2007-11-16 2009-05-21 Thomas Joseph English Continuous Fluid Bed Reactor

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103721664A (en) * 2013-12-13 2014-04-16 中国科学院宁波材料技术与工程研究所 Device and method for modifying carbon material by gas
CN104741062A (en) * 2014-07-09 2015-07-01 季永东 Heat resistant type electrical heating reaction vessel
CN108878766A (en) * 2018-05-22 2018-11-23 桑德集团有限公司 For being modified the device and method of lithium-rich anode material
CN109161226A (en) * 2018-11-02 2019-01-08 巢湖学院 A kind of inorganic nanometer powder surface organic decorating device
CN109161226B (en) * 2018-11-02 2023-07-21 巢湖学院 Inorganic nano powder surface organic modification device

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Application publication date: 20120215